CN105185967A - High-performance carbon-based negative electrode material of lithium ion battery and preparing method thereof - Google Patents
High-performance carbon-based negative electrode material of lithium ion battery and preparing method thereof Download PDFInfo
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- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- H—ELECTRICITY
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- H01M2220/30—Batteries in portable systems, e.g. mobile phone, laptop
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Abstract
The invention provides a high-performance carbon-based negative electrode material suitable for a lithium ion battery and a preparing method thereof. An improved fused salt heating method is used as the preparing method, a three-dimensional structure carbon material having the high specific surface and microtopography at the same time is obtained. The morphology structure is characterized in that a conductive one-dimensional linear carbon material or a conductive two-dimensional sheet-shaped carbon material serves as a framework, and the outer surface of the framework is evenly coated with porous carbon particles. The carbon material serves as the high-performance negative electrode material of the lithium ion battery and has the advantages of being high in mass energy density, good in large-current discharging capacity, long in service life, environmentally friendly and free of heavy metal elements. The preparing method is simple, low in requirement for reaction devices and suitable for industrial production.
Description
Technical field
The present invention relates to high performance carbon based negative electrodes material of a kind of lithium ion battery and preparation method thereof, belong to technical field of lithium ion battery electrode.
Background technology
As a kind of important electrochemical energy storing device, rechargeable lithium ion batteries (rechargeablelithiumionbatteries), at such as mobile phone, achieves huge success in the mobile electronic device of notebook computer etc.But the electronic device of a new generation, as electric automobile, wearable electronic, proposes new requirement to lithium ion battery, simultaneously, along with the development in epoch, the large-scale production of progressively setting up for lithium ion battery of smart electric grid system creates new opportunities and challenges with application.In order to substantially obtain larger breakthrough to the power density of lithium ion battery, energy density, life-span, fail safe, the critical component in lithium ion battery is badly in need of reforming.
Classical lithium ion battery plus-negative plate material system generally with cobalt acid lithium for positive pole, graphite is negative pole.But current commercial graphite negative pole is due to relatively low specific capacity (theoretical capacity 372mAhg
-1), high current charge-discharge poor stability, battery pack safety issue is difficult to solve, and the application in electric automobile power battery runs into bottleneck.In order to address this problem, researcher explores with silicon, tin be representative alloying lithium storage materials and with manganese oxide, iron oxide is the material of the redox storage lithium mechanism of representative.Although these novel materials achieve the raising being several times as much as commercial graphite in specific capacity; but electrode material poorly conductive; in repeated charge process, the inner huge change in volume of electrode material causes battery life to be decayed rapidly; complicated process of preparation, the electrode characteristic shortcoming such as cannot to match with lithium-ion battery system ripe now hinders the actual scale application of these materials greatly.
Consider the height adjustable sex change of carbon-based material in micro-structural and pattern, graphite, as a kind of material with carbon element of simple structure, has great using value to the design of its carbon atom arrangement mode and optimization.Therefore, another kind of effective method is the micro-nano structure carbon material negative pole of exploitation novelty, with alternative conventional graphite Carbon anode.Carbon nano-tube (carbonnanotube) and Graphene (graphene), as novel one dimension, two-dimensional structure material with carbon element, have become the focus of academic circles at present and industrial quarters research.Its high conductivity, the features such as high lithium storage content are very suitable as conductive additive or substrate is applied to negative material.In addition, the porous carbon storing up lithium ability with height carries out compound, can provide new effective way for promoting negative electricity chemical property.To design and to prepare the novel full carbon based negative electrodes material of high electrochemical activity significant to alternative conventional graphite Carbon anode.
Summary of the invention
The object of the invention is to provide a kind of lithium ion battery high performance carbon based negative electrodes material to improve the deficiencies in the prior art, another object of the present invention is to provide the preparation method addressing carbon based negative electrodes material.
Technical scheme of the present invention is: the high performance carbon based negative electrodes material of lithium ion battery, to it is characterized in that on its microcosmic that appearance structure is characterized as conductivity type one dimension wire material with carbon element or two-dimensional sheet material with carbon element is skeleton, porous carbon uniform particles is coated on the material with carbon element in three-dimensional structure that outer surface is formed; Its specific area is 1100-1650m
2g
-1; Described materials application in lithium ion battery negative, at 100mAg
-1current density under, changing into rear discharge capacity (referring to secondary discharge capacity) is 1100-1580mAhg
-1; At 1000mAg
-1high current density under circulation 150 times after capacity be not less than 400mAhg
-1, there is good large current discharging capability and cycle life.
Present invention also offers the method for the above-mentioned carbon based negative electrodes material of preparation, its concrete steps are:
1) by carbonaceous organic material raw material, be dissolved in water-based solvent; The carbonaceous organic material solution A of configuration clarification;
2) by be distributed in water containing one dimension wire material with carbon element or two-dimensional sheet material with carbon element, dispersed with stirring evenly obtains material with carbon element solution B, material with carbon element solution B is joined step 1) in the solution A that obtains, after being uniformly dispersed, at 60-90 DEG C, heating is stirred to gel, obtains the precursor powder of product after drying box;
3) fused salt process of thermal activation is adopted, by step 2) precursor powder that obtains fully mixes with zinc chloride, and roasting under an inert atmosphere, obtains carbon-zinc chloride compound;
4) by above-mentioned steps 3) carbon-zinc chloride compound of obtaining processes in hydrochloric acid solution, washing (zinc chloride in the complex carbon material that removal prepares also reclaims for recycling); The pure material with carbon element obtained carries out drying, obtains the high performance carbon based negative electrodes material of lithium ion battery.
Preferred steps 1) described in carbonaceous organic material raw material be the carbohydrate such as glucose or shitosan; Described water-based solvent is pure deionized water, or adds the acidic aqueous solution after hydrochloric acid, acetic acid or nitric acid; The mass concentration of solution A is 0.5-2.5%.
Preferred steps 2) described in one dimension wire material with carbon element be carbon nano-tube or carbon fiber etc.; Described two-dimensional sheet material with carbon element is graphene oxide or Graphene etc.
Preferred steps 2) described in the mass concentration of material with carbon element solution B be 0.1-0.4%.
Volume ratio when preferred material with carbon element solution B mixes with carbonaceous organic material solution A is 1:(0.75-3).
Preferred steps 3) in the mass ratio of precursor powder and zinc chloride be 1:(5-15).
Preferred steps 3) described in sintering temperature be 400-700 DEG C, roasting temperature retention time is 2-5h.Preferably described protective atmosphere is argon gas or nitrogen.
Beneficial effect:
The invention provides a kind of three-dimensional structure new carbon possessing high-ratio surface and microscopic appearance.The preparing technique process of this product is simple, meets environmental requirement, because production technology significantly reduces the sintering temperature of needs, effectively reduces energy consumption, saved production cost.Product has excellent electrochemistry performance as lithium ion battery negative material, higher than the theoretical capacity of current commercialization graphite cathode, is expected to the lithium ion battery negative material large-scale application of alternative current business-like graphite cathode as a new generation.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope image of the embodiment of the present invention 1 product Graphene/N doping porous carbon;
Fig. 2 is the nitrogen adsorption-desorption curve of the embodiment of the present invention 1 product;
Fig. 3 is the constant current charge-discharge curve of the embodiment of the present invention 1 product as lithium ion battery negative;
Fig. 4 is the scanning electron microscope image of the embodiment of the present invention 2 product carbon nano-tube/N doping porous carbon;
Fig. 5 is the nitrogen adsorption-desorption curve of the embodiment of the present invention 2 product;
Fig. 6 is the constant current charge-discharge curve of the embodiment of the present invention 2 product as lithium ion battery negative;
Fig. 7 is the cycle performance of battery of the embodiment of the present invention 2 product as lithium ion battery negative;
Fig. 8 is the scanning electron microscope image of the embodiment of the present invention 3 product carbon nano-tube/porous carbon;
Fig. 9 is the cycle performance of battery of the embodiment of the present invention 3 product as lithium ion battery negative;
Figure 10 is the scanning electron microscope image of the embodiment of the present invention 4 product Graphene/porous carbon.
Embodiment
Method involved in the present invention comprises but is not limited to the material in following examples.
Embodiment 1: the preparation of Graphene/N doping porous carbon and be assembled into the electrochemical property test of simulated battery.
Be dissolved in 25mL deionized water by 0.7g shitosan, and the watery hydrochloric acid 5mL adding 1mol/L helps to dissolve, abundant stirring and dissolving obtains faint yellow settled solution A, and wherein chitosan concentration is 2.3wt%.Be uniformly dispersed in 40mL deionized water by 50mg graphite oxide, ultrasonic stripping 2h obtains graphene oxide dispersion B, and wherein graphite oxide concentration is 0.12wt%.Solution A and dispersion liquid B are uniformly mixed and spends the night, after heating is stirred to gel at 90 DEG C, dries completely in air dry oven and obtain presoma powder.Get after 0.4g presoma mixes completely with 4g zinc chloride powder, 600 DEG C of roasting 2h under argon atmosphere, remove the slaine impurity in material completely, obtain end product after oven dry with the watery hydrochloric acid of 1mol/L and deionized water cyclic washing after Temperature fall.Microstructure as shown in Figure 1, can find out N doping porous carbon uniform load that shitosan carbonization the obtains graphenic surface in sheet.The nitrogen adsorption desorption curve shows material of Fig. 2 has abundant microcellular structure, calculates specific area and reaches 1626m
2g
-1.
The sample prepare above-mentioned example 1 and conductive black, binding agent (PTFE) than Homogeneous phase mixing, prepares electrode slice according to 8:1:1 quality.With 2025 type button cells for test system, metal lithium sheet is to electrode, and electrolyte uses the 1MLiPF be dissolved in organic solvent
6, in the glove box of argon shield, be assembled into lithium ion battery, and test performance (in following case study on implementation, prepare simulated battery step if no special instructions, method is namely identical with foregoing description).High accuracy battery tester is investigated lithium ion battery negative material performance.Recording current density is 100mAg
-1time charging and discharging curve as Fig. 3, material second time discharge capacity be 1553mAhg
-1, reach current commercialization graphite cathode theoretical capacity (372mAhg
-1) 4 times, at 1000mAg
-1high current density under circulation 150 times after capacity be 468mAhg
-1.
Embodiment 2: the preparation of carbon nano-tube/nitrogen-doped carbon composite material and be assembled into the electrochemical property test of simulated battery.
Be dissolved in 115mL deionized water by 0.7g shitosan, and the watery hydrochloric acid 5mL adding 1mol/L helps to dissolve, abundant stirring and dissolving obtains faint yellow or colourless settled solution A, and wherein chitosan concentration is 0.58wt%.50mg carbon nano-tube is uniformly dispersed in 40mL deionized water and obtains dispersion liquid B, wherein carbon nanotube concentration is 0.2wt%, solution A and dispersion liquid B are uniformly mixed and spends the night, after heating is stirred to gel at 80 DEG C, dries completely in air dry oven and obtain presoma powder.Get after 0.4g presoma mixes completely with 4g zinc chloride powder, 600 DEG C of roasting 2h under argon atmosphere, remove the slaine impurity in material completely, obtain end product after oven dry with the watery hydrochloric acid of 1mol/L and deionized water cyclic washing after Temperature fall.Microstructure as shown in Figure 4, can find out carbon nano-tube intert the N doping porous carbon body that obtains in shitosan carbonization mutually in, form three-dimensional conductive structure, contribute to electronics height storage lithium activity N doping porous carbon body mutually in conduction.In Figure 5, nitrogen adsorption desorption curve shows material has abundant micropore and mesoporous, and calculating specific area is 1420m
2g
-1.After material is assembled into lithium ion battery, test its lithium ion battery negative performance.Fig. 6 and Fig. 7 illustrates respectively, at 100mAg
-1current density under material secondary discharge capacity can reach 1168mAhg
-1, and at 1000mAg
-1large charging or discharging current under circulation 150 times after capacity still up to 492mAhg
-1, circulation coulombic efficiency is close to 100%.
Embodiment 3: the preparation of carbon nano-tube/porous carbon composite and be assembled into the electrochemical property test of simulated battery.
Be dissolved in by 0.7g glucose in 50mL deionized water, abundant stirring and dissolving obtains colourless settled solution A, and wherein concentration of glucose is 1.4wt%.50mg carbon nano-tube is uniformly dispersed in 40mL deionized water and obtains dispersion liquid B, wherein carbon nanotube concentration is 0.12wt%, solution A and dispersion liquid B are uniformly mixed and spends the night, after heating is stirred to gel at 90 DEG C, dries completely in air dry oven and obtain presoma powder.Get after 0.4g presoma mixes completely with 6g zinc chloride powder, 700 DEG C of roasting 3h under pure nitrogen gas atmosphere, remove the slaine impurity in material after Temperature fall completely with the watery hydrochloric acid of 1mol/L and deionized water cyclic washing, obtain end product after oven dry, pattern as shown in Figure 8.Material specific surface area is 1320m
2g
-1.The porous carbon obtained by glucose carbonization is more loose porous, becomes foam-like to be carried in carbon nano-tube and forms three-dimensional structure.After material is assembled into lithium ion battery, test its lithium ion battery negative performance, Fig. 9 describes material at 100mAg
-1current density under, secondary discharge capacity is 1396mAhg
-1, the capacity after 40 times that circulates still can remain on 1113mAhg
-1, there is high storage lithium performance.And at 1000mAg
-1large charging or discharging current under circulation 150 times after capacity be 425mAhg
-1.
Embodiment 4: the preparation of Graphene/porous carbon composite and be assembled into the electrochemical property test of simulated battery.
Be dissolved in by 0.7g glucose in 100mL deionized water, abundant stirring and dissolving obtains colourless settled solution A, and wherein the concentration of glucose is 0.7wt%.Be uniformly dispersed in 40mL deionized water by 160mg graphite oxide, ultrasonic stripping 2h obtains graphene oxide dispersion B, and wherein graphene oxide concentration is 0.4wt%.Solution A and dispersion liquid B are uniformly mixed after spending the night, after heating is stirred to gel at 60 DEG C, dries completely in air dry oven and obtain presoma powder.Get after 0.4g presoma mixes completely with 2g zinc chloride powder, 400 DEG C of roasting 5h under pure nitrogen gas atmosphere, remove the slaine impurity in material completely, obtain end product after oven dry with the watery hydrochloric acid of 1mol/L and deionized water cyclic washing after Temperature fall.The specific area that test obtains material is 1172m
2g
-1.Figure 10 describes the porous carbon that glucose carbonization obtains and is evenly supported on graphene sheet layer, the Graphene of sheet is wrapped completely, and to observe porous carbon be loose and porous structure, this comparatively open three-dimensional carbon structure is conducive to improving the diffusion rate of lithium ion in negative material, makes lithium ion battery negative have higher performance.After material is assembled into lithium ion battery, test its lithium ion battery negative performance, material is at 100mAg
-1current density under, secondary discharge capacity is 1120mAhg
-1, and at 1000mAg
-1large charging or discharging current under circulation 150 times after capacity be 409mAhg
-1, illustrative material high rate performance is better.
Claims (8)
1. the high performance carbon based negative electrodes material of lithium ion battery, is characterized in that for conductivity type one dimension wire material with carbon element or two-dimensional sheet material with carbon element are skeleton, and porous carbon uniform particles is coated on the material with carbon element in three-dimensional structure that outer surface is formed; Its specific area is 1100-1650m
2g
-1; Described materials application in lithium ion battery negative, at 100mAg
-1current density under, changing into rear discharge capacity is 1100-1580mAhg
-1; At 1000mAg
-1high current density under circulation 150 times after capacity be not less than 400mAhg
-1.
2. prepare a method for carbon based negative electrodes material as claimed in claim 1, its concrete steps are:
1) by carbonaceous organic material raw material, be dissolved in water-based solvent; The carbonaceous organic material solution A of configuration clarification;
2) by be distributed in water containing one dimension wire material with carbon element or two-dimensional sheet material with carbon element, dispersed with stirring evenly obtains material with carbon element solution B, material with carbon element solution B is joined step 1) in the solution A that obtains, after being uniformly dispersed, at 60-90 DEG C, heating is stirred to gel, obtains the precursor powder of product after drying;
3) fused salt process of thermal activation is adopted, by step 2) precursor powder that obtains fully mixes with zinc chloride, and roasting under an inert atmosphere, obtains carbon-zinc chloride compound;
4) by above-mentioned steps 3) carbon-zinc chloride compound of obtaining processes in hydrochloric acid solution, washing, dry, obtains the high performance carbon based negative electrodes material of lithium ion battery.
3. method according to claim 2, is characterized in that step 1) described in carbonaceous organic material raw material be glucose or shitosan; Described water-based solvent is pure deionized water, or adds the acidic aqueous solution after hydrochloric acid, acetic acid or nitric acid; The mass concentration of solution A is 0.5-2.5%.
4. method according to claim 2, is characterized in that step 2) described in one dimension wire material with carbon element be carbon nano-tube or carbon fiber; Described two-dimensional sheet material with carbon element is graphene oxide or Graphene.
5. method according to claim 2, is characterized in that step 2) described in the mass concentration of material with carbon element solution B be 0.1-0.4%.
6. method according to claim 2, is characterized in that volume ratio when material with carbon element solution B mixes with carbonaceous organic material solution A is 1:(0.75-3).
7. method according to claim 2, is characterized in that step 3) in the mass ratio of precursor powder and zinc chloride be 1:(5-15).
8. method according to claim 2, is characterized in that step 3) described in sintering temperature be 400-700 DEG C, roasting temperature retention time is 2-5h.
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| CN107017091B (en) * | 2017-04-25 | 2018-11-23 | 武汉大学 | Nitrogenous multistage porous carbon/graphene composite material and its preparation method and application |
| CN110627033A (en) * | 2018-06-22 | 2019-12-31 | 武汉大学 | Nitrogen and sulfur co-doped multistage porous carbon composite material and preparation method and application thereof |
| CN110416522A (en) * | 2019-08-02 | 2019-11-05 | 上海汽车集团股份有限公司 | A kind of composite negative pole material containing lithium, preparation method and its application in the lithium secondary battery |
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